Peogbss of and apparatus fob treatment op bituminous materials



April`2, 1929. w. H. HAMPTON PROCESS OF AND APPARATUS FOR TREATMENT OFBITUMINOUS MATERIALS QJ, 2 Sheets-Sheet Filed Dec. 17, 1919 2 Sheets-Sheet 2 April 2, 1929. w. H. l-IMHQTONl PROCESS OF AND APPARATUS FOR TREATMENT 0F BITUHINOUS MATERIALS Filed Dec; 17, 1919` Hw www,

Patented Apr. 2, 1929.

PATENT FFICE.

VTLLIAM HUNTLEY HAMPTON, OF PORTLAND, OREGON.

OF AND APPARATUS FOR TREATMENT 0F BITUMNOUS MATERIA-.

Application lcd December 17, 1913.

This invention relates to processes of andv apparatus ifor treatment oi bituminous materials. in oaricula Lhe invention has to do r ,v tie l o shale or other bitumini'ierou. -ds tor the purpose of obtaining valuable iydrocarbons therefrom. ienerallif described, the process involves diges- Lolii the bituminous material to be treated l i a. hrdrocarlfion solvent or digest' '1g me- 'um u der pressure, coupled with a simulif-.ous refiningI treatment ot such hydrobon vapors as may be evolved during the 'estiong and the residual digestion mi):- ture being then treated Yfor separation of solid materia trom the accompanying unvaporized L lfeaturo oit the invention as practiced .in one ot its advantageous Yforms the employr'ent ot a digestion solvent which, at ordinary atmospheric pressure, would be wholly or largely vaporized at the digestion temperatures used, but which is to a grr-at extent prevented from so vaporizing bv the pressure under which the digestion apparatus is maintained. By enniloying` a hydrocarbon solvent of this character, that is to say, an oil Ytraction lighter or ot higher laume than a lubricating; traction, and by employing such relatively light 'tractioirin suilioiently large proportion in mixture with the bituminous material to be treated, the 1-1iii -1eq nent se@ `'ation ot solid material trom the residual o gestion mixture may be very much simplified and iiiacilitated, as will hereinafter appear. At the same time, vaporii/.atien o'tljinhter iractions during the dil.egesiimi is not entirely suppressed, and may in 'fact be encouraged to a certain extent; and the re-:ultant vapors may he led away and subiected to suitable treatment .tor production o? desired 'traction-s, simultaneously with tl e pro ss oi the digestion. By employing suitable apparatus. the entire seres ot operations mn he effected economically in a continuous` manner with the production of prac- 1riraily no free carbon or coky residues such as charaetiuiUe most ordinary methods for treating: materials oit the` character here in question.

lli/while the invention is not limited in its application to treatment oit any speeiic bituminous: material, it linds its greatest present utilitaT in the treatment ot shale and other oil-henriug rock or bituminil'erous solid materials generally; and Y.tor the purpose of fully fpiaining the underlying principles ot the Serial No. 345,485.

in *cntiom the treatment of bituminous shale will therefore be more particularly reterred to. Suitable apparatus of novel character will also he described in connection .vith the carrying out ot the process in practice, although it to be understood that the process may be practiced in other Yforms of apparatus than that hereinafter described. Typical norel apparatus suitable for carrying` out the process is illustrated in the accompanying' drawings in Which Figs. l and 2 represent, more or less diai;rammatically, a complete plant in side elevation, partly in section; and

Figs. 3 and f1'- `are fragmentary plan views ot parts of said system.

ln the particular embodiment oit the novel process here chosen tor purposes ot illustration, oil-bearing` shale, crushed to say one- Yi'f'ourth inch mesh, is ted Yfrom a source ol supply at l() into a combined heater and mixer 1l, where it thoroughly mixed with a relatively iight mineral oil fraction, such as a kerosene, which is ted to the mixer ll ix'rom one or the other ot' the tanks l2, 13, through a pipe l-l, which has a preheating coil l5 located Within an enlargement 1G ot a llue leading trom the furnace 1i' below the combined heater and mixer 1l. oi crushed shale and preheated kerosene is advanced by a series ot conveyors 18 through the mixer. and is discharged at say from 3000 to 400 F. into grinding apparatus, which in this instance comprises a ball mill or tube mill i9, which may be enclosed in brickWoi-k or the like 20 and maintained at the specilied temperature by suitable heating means, it necessary. At this toinperature it 1s a comparatively simple matter to reduce the crushed shale to avery iinely pulverulent condition, although 'when cold, it is difficult to pulverize. ln practice, the shale should most advantageously be ground at this stage until or more vvill pass a 20() mesh sieve. T he proportion o1"A kerosene or other light traction may vary considerably, but should be such as to ve a readily fluent mixture when the `grinding;v is. completed. ln practice an adiiition ot kerosene in the proportion of one volume of kerosene to one volume oll shale, is Jfound to five satisfactory results. lllhere the oil traction en'iployed a solvent in adinifiture with the shale is so light as to volat-ilize considerably at the temperatures employed .in the mixer and grinder, suitable or or not the digestion has been carried far enough. In the course oi this somewhat prolonged digestion, not only are valuable bitun'iens dissolved from the solid material, but the liquid portion or the mixture experiences more or less breaking down and rearrangement ci" the heavy hydrocarhou compounds contained therein, especially in the pressure digester. This breaking down or rearrangement, While perhaps more or less analogous to so-called cracking iin certain respects, nevertheless diilfers substantially trom what is conunonly tnown as cracking, in that the transtormations or conversions undergone are apparently in the nature of a smooth molecular splitting which does not involve the 'tree carbon or gas to a material lily virtue of this fact, no difficulty experienced trom deposits oi" coke or carbon in the retorts; nor is there the, high .loss in l'ixed gas characterizing what are comvnionly tcrn'ied cracking processes. Nevertheless the erosene, or other traction heavier than gasoline, employed as the digestion solduring the digestion, apparently undergoes the aforesaid splitting or cleaving reactions to a considerable er. ent, with the resultant production et lighter products of the nature ot gasoline contained in the dieestion vapors, all oiI which are suitably led oli", into the main vapor pipe El, tor example., ter 'further treatment to he hereinatter described. vWhere kerosene is the digestion medium, the digestion vapors also contain more or less unchanged kerosene, depending upon the temperatiju'e and 'duration of the digestion, such volatilized kerosene consisting partly of that originally added and partly of Vthat derived :from the shale. But, as hetero stated, the vaporization should he carefully regulated in order that it may not become excessive, and in order that the linal digestion mixture may he oit the proper degree oi" fluidity.

Atteithe digestion is complete, it is necessary to separate residual solid matter from the acconuknrnying unvaporized oil consisting of oil ot di gestion and oils, waxes, etc., including lubricating 'fractions derived trom the hitun'iinous material, and this may loe effected in various ways. `Wliatever method of separation he eiuployed, ,it is advisable first to cool down the digestion mixture considerably heiiore .making the separation. To this end, the digestion niixture is discharged from the pressure retort 23 into a suitable cooleror heat exchanger eil. Said heat exchanger' should also he maintained under pressure in order to prevent undue vaporization of lighter fractions troni the hot mixture Which it receives. This pressure may he maintained substantially the same as in the pressure retort hy proper adjustment oit valve 42 in the vapor pipe 43 with which the cooler Lll is provided and which may lead into the main vapor pipe 8l. lVithin this heat exchanger, the digestion mixture is mace to ,give up large part of its heat to considerably cooler oil derived trom a later stage of the process, as Will he, explained presently.

ln the present instance separation ot the solid matter troni the residual digestion mixture etlected centritugally, and most desirahly hy centri'lfugal iltration; and the conditions o operation are so regulated and controlled that this centrifugal .eparation may he carried out Without thinning down or diluting the digestion mixture with kerosene or other light mineral oil traction. Accordingly, it the digestion has properly conducted, the digestion mii yure still contains such a large proportion ci erosene that even when. it cooled down 'to say l0() to Q00" F., which is a suitable temperatinfe tor the centrifugal separation, it is still su'iciently fluid to enalole satisfactory separa-tion Without dilution. Since the, cooler or heat exchanger lil :is maintained under pressure, as described, and since it is most convenient to eiiect the centrifugal separation at ordinary atmospheric pressure, it necessary to provide a lock system or the like, 441, dat, similar to 32, 3", i'or transferring the cooled di gestion mixture from the heat exchanger to the centrifugal separator or .filtering device 115. by closing discharge valve ilG and also valve 47 in vapor outlet 48, it open), and openingvalve 4:9 in cqualizing pipe 50, and discharge valve 5l, digestion mixture nioved into the discharge outlet 52 by the Conveyor in the heat exchanger, may he discharged into vessel 44 o1"- the lock system, which will [ill to the level 0l.l the liquid in the heat exchanger il. By new closing valves 4:2) and 5l, and opening valve 46, the mixture in L' /l may he gravitally discharged to the centriA igal, solid matter being caught on the rotating screen or basket thereof, and separated oil passing through pipe 53 to a receiving` tank rllhe two passages dal, and del oit the locking-out system are oit course operated in alternation in a manner similar to the locking-in system 32, 32, so that continuous operation is possible. Solids retained on the centriiiu gal screen may he Washed iliree oil heavy oils, etc., it desired, hy Warm kerosene or other light solvent supplied from tank 55 through pipe 56, the Washings also going to tank 5%.

Atter- Washing on the centrifugal screen, the retained solids may he dropped into a drier 57 from which kerosene or other vapors may he led off through pipes 5S and 59 Yfor recovery by condensation and returned to supply tank 55, by means not shown. 'A he dried solid matter may he discharge fl troni the drier at GO, and it suiliciently exhausted of valuable -bituminous matter, may he discarded; otherwise such solids may he suhlll) jected to further treatment iter recovery oit residual lnitun'iens7 in any Suitable nntnncr unnecessary to describe here.

The oil Collected in the receiving;` tnnlc 5%-, 'which is a mixture ot light find. heavy tractious, is suhjectod to suitnhle tractionation lor separation into desired p 'oducts rThis mixture heilig relatively cool, inust he heated to ellleet 'ti-actiouation. 'llo this end it is ''orced hy pump Gl through pipe G2 .into heetreceiriugi felation to the hot digestion oil. in tho heut exchanger or cooler l-l. in this iuetzuice the relatively cool oil pass-es trein pi pe (3:2 into a series oit pipo hends (53 arraiured in contact with the outside ot the loner part ot the dino/:1itel shell, which may he et sheet metal in nrcori'lnnce with the usual construction ol oil retorts or stills. ri`he said lower part o'l the heut exchanger shell, where not eufralg'ed hy the coils (33, .may he protected hy heat insulation (3ft, it desired. litter p: sfr ing; through the hcnds (33, the cooling oil passes through pipe (35 into hoods Gli, which ure ar angled inside the heat exchanger and helow the liquid level therein. ngliler puse ini;` througggh hends (353 und Gti, the oil mixture is relatively hot hut it not sulliciently hot iior 'tractionating purposes, it may he lurthi-,r healed hy menus, not shown7 to the necessary toinpcratlirc. ln any event, the hot oi] .is mientually diisiirhzuged through pipe hl into a rose (38, hy n'ieans ot which it is sprayed into the upper pnrt ot a topijing tower (Vak iu which the lighter tractious ure valviorzed and pass otl through outlet into z, series ot comlensing),` ehumhers 7l, TL, etc., `from which various tractions ma); he separatelj,y drawn ollf through outlets 73, Tl, etc. Assuming that a kerosene traction is col looted in Tl, this may he drnrvix 'trein the coin mou collol-line4 main T5 hy pump ih and sont thi-(nigh pipe-i7 to sirpiihr tuoi; 'l-l 'tor eX- :imple7 t he vulves in seid collecting main heini; ot course munipuluted to allow the pump to draw exclusively the l'rnction deposited in rhamhor Tl. ln case it uur); also he desired lo employ heavier oil lor digestion, with the apliuiratus desrrihed7 the pump 7G may also he uned to draw such heavier oil .troni the hase ot the topping tower (Si) and torce it throi'lgh pipe 7i and l) anch i3 to the supply tank l2, the various valves shown in the piping;l sys lem heini; adire-:teal to permit this.

`vapors evolved :trom the digestion rel'zorts und other piu-s et the apparatus having' vapor pipes conrmcted to the main vapor pige 3l are suhieotml to tui'ther tr iatmeutv7 as staleifl, to ohtain therefrom desired valuable productsa ,ln the ine-aout exemple, the vapers contain hot-h gasoline and lnfrosene 'trucionf-i, and it is desired to treat this mixture tor )reduction ot e lzuger proportion ot gms oline than is initially contained therein. To this end` `steam mixed with the apors and the comhinutiou is then subjected to tempermorirse ntures substantially higher than those einployed in the digestion, in order to ettect cracking, the presence ol the steam in the mixture serving to prevent extensive ternir tion of 'tree carbon and ecky products in the cinclning` apparatus. Various torus ot er: :hing apparatus may he employedj hut in the example here illijlstrated, the vapors nre dra rn hy steuni injectorl 7S) :from vapor pipe 3l, und the mixture forced at high velocity through coils ot metal piping' 80 and hl heated lo u maxi muni tenuerature ot nrouud 1300 degrees lhlv or thererhouts, by any suitable liriny means such its gais or oil burners 82. nur heavy liquid matter7 such as heavy oil@l or tu s collecting in the c 'achingl coils may he t 'zipped ott through valved pipes 83 and conveyed through :t Common down pipe ce to a receiver 85, to he disliiosetl oit in any desired lnannef. The cracked vapors leave the crau-kinIg)v retort system at S6, and enter a' condensing und ifractiomttingsystem, coinprif-ainn' in this instance two sets oli condensingu towers or chambers 87, 88, and S9, 90. Although tour such chambers a-re shown, the system may ot course comprise as many chzuuher.` as may he necessary to produce the 'lruetionifi desired. The conditions may he adiusted so that heavier fractions such is luhrirating oils und heavier lteroseucs ure ehtzsined in rinidensers 87, and S8, while lighter ilrmitions, imiiluding` light kerosenes unil gnsolines, are obtained, in t3?) und 90, or in succeei'liug chalutiers, not shown. lfu order JVo ohtaiu suhs'tztntially colorless light 'herosene and gasoline 'tract/ions, without extensive subsequent -lvnuiticatimi and retining` lreutluenh it hns been tound desi idole in practice to interpose between condensers S8 and 99 a vnsher 91 into which vapors com inn' trom condenser 88 through pipe 92 are huhhled through wzitor 93 in the Washer and n e caused to deposit any contained tari-y :ind coloring mutter or `the like, together with some herosenes, which may .he 1withalrawn tl'uoun'h outlet 9N; While the cleansed vapors oft the `kerosene and gasoline tractions pass on through pipe ffl-fl into the succeeding series 'it condensingy chzunhers.

Tdlluit l claim is:

l. The pr )cess ot obtaining` valuable hydrmznrhon products which coniiirises mixing; with lfiitiuninous slutle-like solid metter, .fr lniiieral oil having' a nvity Within the kerosene ronge, digestine` the n'iixture :it a ternperutu re hi gli enough to lique'ly contained hituincns und under su'liicient pressurelto suhslantinlly retaixfl vaporizntion oli Jthe keros-sne and heavier fractions7 conducting away und recovering volntilized products, and sepuratingY solid matter from the residual digested mixture.

2. Vlllhe process ot obtaining ifnluahle hydrocarbon products which comprises digestinn` u mixture ot a ke osene gravity mine al oil and finely divided bituminous shale-like solid metter at from 500 to 7000 F. and under i)i'cssui'e, the pressure employed. beiner hijerh enough t-o suppress Vaporization of the kerosene fraction to such an extent that the solids present in the mixture remainingV after digestion nre separable centrifugally Without dilution, conducting` away and recovering.;v volatilized products, find centrifugally separating solid matter from the residual dilrested mixture.

5:3. The process oi? obtaining` valuable liydrocarbon products which comprises digesting a mixture of bituminous shale-like solid mattei.' with a hydrocarbon oil under pressure and at temperatures high enough to extract contained bitumens, but not high enough to distill olif lubricating or heavier oil iractions to a substantial e.\ l nt, obtaining); valuable products from the digestion vapors, and separating solid matter from the residual {iuid digestion mixture.

Il. rl`he process o1 obtainingvaluable hyy drocarbon products which con'iprises digesting a mixture of bituminous shale-like solid metter with. a hydrocarbon oil having a gravity within the kerosene range at teinperatures high enough and for a sufficient length of time to extract contained bitmnens andv to effect substantial breaking-down or conversion of heavy hydrocarbons into lighter, but avoiding temperatures high enough to proifluce substantial formation ol free curbon or coke, leading oi evolved vapors and obteining.;i valuable product, tlnirefroin, :ind separating solid mattei' from the residual l'iuid digestion mixture.

The prec ss el obtaining' valuable hydrocarbon products, which comprises digesting a mixture of bituminous shale-like solid matter with a hydrocarbon oil first at a pressure not substantially exceeding' atmospheric and then under superatmospheric pressure, the temperature being higher in the letter stage and suliiciently high to extract contained bitumens, recovering;` valuable products 'from the vapors evolved. during digestion, and separating; solid mutter 'from the residual. lluid dieestion mixture.

(i. rlipparatus Ier treating' bituminiiferous materials comi risingij, in ceinbimition, a plurality of digesters, ineens for :ulvancing` materia-l through said digestersi; vsuccessively in seri-es, the lest digester in the series being' Aadapted for operation under sulieratinospheric pressure, a` cracking retort connected to seid digesters sind arranged to receive vapors there'lrom, and liquid-separating means connected to the pressure digester and. arranged vto trent the mixture of solid. and liquid material coming' therefrom.

In testimony whereof I hereunto afiix my signature.

VWM. HUNTLEY HAMPTON. 

